EP1149893B1 - Wäscheweichspülmittel enthaltende Dosierungseinheit zur Verwendung in einem Waschgang - Google Patents

Wäscheweichspülmittel enthaltende Dosierungseinheit zur Verwendung in einem Waschgang Download PDF

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Publication number
EP1149893B1
EP1149893B1 EP00203113A EP00203113A EP1149893B1 EP 1149893 B1 EP1149893 B1 EP 1149893B1 EP 00203113 A EP00203113 A EP 00203113A EP 00203113 A EP00203113 A EP 00203113A EP 1149893 B1 EP1149893 B1 EP 1149893B1
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EP
European Patent Office
Prior art keywords
softening
unit dose
composition
pentaerythritol
fatty
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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EP00203113A
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English (en)
French (fr)
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EP1149893A1 (de
Inventor
Alain Jacques
Hoai-Chau Cao
Juliette Rousselet
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Colgate Palmolive Co
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Colgate Palmolive Co
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Publication date
Priority claimed from US09/558,822 external-priority patent/US6258767B1/en
Application filed by Colgate Palmolive Co filed Critical Colgate Palmolive Co
Priority to EP05076606A priority Critical patent/EP1586626A3/de
Publication of EP1149893A1 publication Critical patent/EP1149893A1/de
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Publication of EP1149893B1 publication Critical patent/EP1149893B1/de
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246—Silicates, e.g. diatomaceous earth
    • C11D3/1253—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
    • C11D3/126—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite in solid compositions
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66—Non-ionic compounds
    • C11D1/667—Neutral esters, e.g. sorbitan esters
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047—Detergents in the form of bars or tablets
    • C11D17/0065—Solid detergents containing builders
    • C11D17/0073—Tablets
    • C11D17/0086—Laundry tablets
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/04—Detergent materials or soaps characterised by their shape or physical properties combined with or containing other objects
    • C11D17/041—Compositions releasably affixed on a substrate or incorporated into a dispensing means
    • C11D17/042—Water soluble or water disintegrable containers or substrates containing cleaning compositions or additives for cleaning compositions
    • C11D17/044—Solid compositions
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/0005—Other compounding ingredients characterised by their effect
    • C11D3/001—Softening compositions

Definitions

  • This invention relates to wash cycle unit dose laundry compositions for softening or conditioning fabrics. More particularly, this invention relates to unit dose fabric softening compositions which are compacted granular compositions or encapsulated liquid or granular compositions suitable for use in the wash cycle of an automatic washing machine.
  • Detergent compositions manufactured in the form of compacted detergent powder are known in the art.
  • U.S. 5,225,100 describes a tablet of compacted powder comprising an anionic detergent compound which will adequately disperse in the wash water.
  • detergent compositions in the form of compacted granular tablets of various shapes have received much attention in the patent literature, the use of such tablets to provide a unit dose fabric softener which will soften or condition fabrics in the wash cycle without impairing detergency or otherwise compromise the cleaning benefits provided by the detergent composition is not known.
  • a unit dose composition for the rinse cycle must be formulated to readily dispense its contents upon contact with water in a period of time corresponding to the residence time of the unit dose in the dispenser, namely, the period of time during which water enters and flows through the rinse cycle dispenser.
  • Laundry detergent compositions which further include a fabric softener to provide softening or conditioning of fabrics in the wash cycle of the laundering operation are well-known in the art and described in the patent literature. See, for example, U.S. Patent 4,605,506 to Wixon ; U.S. Patent 4,818,421 to Boris et al. and U.S. Patent 4,569,773 to Ramachandran et al. , all assigned to Colgate-Palmolive Co., and U.S. Patent 4,851,138 assigned to Akzo .
  • U.S. Patent 5,972,870 to Anderson describes a multi-layered laundry tablet for washing which may include a detergent in the outer layer and a fabric softener, or water softener or fragrance in the inner layer.
  • wash cycle active fabric softeners typically in powder form. But, these type products are characterized by the same inconvenience inherent with the use of powered detergents, namely, problems of handling, caking in the container or wash cycle dispenser, and the need for a dosing device to deliver the desired amount of active softener material to the wash water.
  • EP Patent 530 958 describes a fabric softening composition which can be used in the wash cycle and comprises a granular or liquid product comprising a montmorillonite-containing softening clay and a higher aliphatic acid ester of pentaerythritol. It has now been found that softening of laundry can be effected in the wash cycle with a flexibility which is independent of the detergent dosage, and with great convenience by the consumer by the use of a unit dose wash cycle softener which avoids the common problems associated with the pouring and handling of granular or liquid detergent compositions.
  • the present invention provides a unit dose wash cycle fabric softening composition according to claim 1.
  • the unit dose fabric softening composition is characterized by being in the form of a tablet and having no discrete outer layer surrounding the fabric softener comprised of an alkaline material such that the pH of the wash water is increased upon dissolution of said outer layer in said wash water.
  • granular as used herein in describing the fabric softener is intended to encompass relatively coarser granules varying in size from about 150 to 2,000 microns as well as finer powder having a size as small as 30 to 50 microns.
  • fabric softener is used herein for purposes of convenience to refer to materials which provide softening and/or conditioning benefits to fabrics in the wash cycle of a home or automatic laundering machine.
  • the compacted granular fabric softener composition of the invention is preferably comprised of a fabric softening clay optionally in combination with an organic fatty softening material.
  • a fabric softening clay optionally in combination with an organic fatty softening material.
  • Especially preferred fabric softeners comprise a clay mineral softener, such as bentonite, in combination with a pentaerythritol ester compound as further described herein.
  • Useful combinations of such softener may vary from about 80%, to about 90%, by weight, of clay, and from about 10% to about 20%, by weight, of fatty softening material such as a pentaerythritol compound (often abbreviated herein as "PEC").
  • PEC pentaerythritol compound
  • the encapsulated liquid or granular fabric softener composition contemplated for use herein comprises a gelatin capsule containing a nonionic softener or clay to avoid any reaction with anionic surfactants which may be present in the wash liquor.
  • useful liquid softening compositions include fatty alcohols, fatty acids, fatty esters, silicones (e.g. linear, grafted, crosslinked or ethoxylated), polyethylene waxes and fatty amides.
  • a process for softening or conditioning laundry which comprises contacting the laundry with an effective amount of the unit dose laundry composition defined above.
  • the clays that are useful components of the invented products are those which cooperate with the organic fatty softener materials to provide enhanced softening of laundry.
  • Such clays include the montmorillonite-containing clays which have swelling properties (in water) and which are of smectite structure, so that they deposit on fibrous materials, especially cotton and cotton/synthetic blends, such as cotton/polyester, to give such fibers and fabrics made from them a surface lubricity or softness.
  • the best of the smectite clays for use in the present invention is bentonite and the best of the bentonites are those which have a substantial swelling capability in water, such as the sodium and potassium bentonites.
  • Such swelling bentonites are also known as western or Wyoming bentonites, which are essentially sodium bentonite.
  • Other bentonites such as calcium bentonite, are normally non-swelling and usually are, in themselves, unacceptable as fabric softening agents.
  • a source of alkali metal or other solubilizing ion such as sodium (which may come from sodium hydroxide, added to the composition, or from sodium salts, such as builders and fillers, which may be functional components of the composition).
  • bentonites are those of sodium and potassium, which are normally swelling, and calcium and magnesium, which are normally non-swelling. Of these it is preferred to utilize calcium (with a source of sodium being present) and sodium bentonites.
  • the bentonites employed may be produced in the United States of America, such as Wyoming bentonite, but also may be obtained from Europe, including Italy and Spain, as calcium bentonite, which may be converted to sodium bentonite by treatment with sodium carbonate, or may be employed as calcium bentonite.
  • other montmorillonite-containing smectite clays of properties like those of the bentonites described may be substituted in whole or in part for the bentonites described herein and similar fabric softening results will be obtained.
  • the swellable bentonites and similarly operative clays are of ultimate particle sizes in the micron range, e.g., 0.01 to 20 microns and of actual particle sizes in the range of No's. 100 to 400 sieves, preferably 140 to 325 sieves, U.S. Sieve Series.
  • the bentonite and other such suitable swellable clays may be agglomerated to larger particle sizes too, such as 60 to 120 sieves, but such agglomerates are not preferred unless they include the PEC('s) too (in any particulate products).
  • a main component of the invented compositions and articles of the present invention, and which is used in combination with the fabric softening clay is an organic fatty softener.
  • the organic softener can be a higher aliphatic acid ester of pentaerythritol an oligomer of pentaerythriol, a lower alkylene oxide derivative of pentaerythritol, an oligomer of and a mixture thereof.
  • Pentaerythritol compound is often abbreviated as PEC herein.
  • the oligomers of pentaerythritol are preferably those of two to five pentaerythritol moieties, more preferably 2 or 3, with such moieties being joined together through etheric bonds.
  • the lower alkylene oxide derivatives thereof are preferably of ethylene oxide or propylene oxide monomers, dimers or polymers, which terminate in hydroxyls and are joined to the pentaerythritol or oligomer of pentaerythritol through etheric linkages.
  • At least one of the PEC OH groups and preferably at least two, e.g., 1 or 2 to 4 are esterified by a higher fatty acid or other higher aliphatic acid, which can be of an odd number of carbon atoms.
  • the higher aliphatic acid esters of the pentaerythritol compounds are preferably partial esters. And more preferably there will be at least two free hydroxyls thereon after esterification (on the pentaerythritol, oligomer or alkoxyalkane groups). Frequently, the number of such free hydroxyls is two or about two but sometimes it may by one, as in pentaerythritol tristearate.
  • the higher aliphatic or fatty acids that may be employed as esterifying acids are those of carbon atom contents in the range of 8 to 24, preferably 12 to 22 and more preferably 12 to 18, e.g., lauric, myristic, palmitic, oleic, stearic and behenic acids.
  • Such may be mixtures of such fatty acids, obtained from natural sources, such as tallow or coconut oil, or from such natural materials that have been hydrogenated. Synthetic acids of odd or even numbers of carbon atoms may also be employed. Of the fatty acids lauric and stearic acids are often preferred, and such preference may depend on the pentaerythritol compound being esterified.
  • pentaerythritol compounds that are useful in the practice of this invention are illustrated it will be understood that various other such pentaerythritol compounds within the description thereof may also be employed herein, including such as pentaerythritol dihydrogenated tallowate, pentaerythritol ditallowate, pentaerythritol dipalmitate, and dipentaerythritol tetratallowate
  • the organic softening material can also be a fatty alcohol.
  • cationic softeners such as conventional quaternary ammonium softening compounds may optionally be added in minor amounts.
  • the combination of bentonite and organic fatty softening material is generally from about 10% to about 100% bentonite and from about 1% to about 100% fatty softening material, preferably from about 50% to about 95% bentonite and about 5% to about 50% fatty softening material, and most preferably from about 80% to 90% bentonite and from about 10% to about 20% fatty softening material.
  • compositions of the invention include disintegration materials to enhance the disintegration of the unit dose in the wash water.
  • materials include an effervescent matrix such as citric acid combined with baking soda, or materials such as PVP polymer and cellulose.
  • Granulating agents may be used such as polyethylene glycol; bactericides, perfumes, dyes and materials to protect against color fading, dye transfer, anti-pilling and anti-shrinkage.
  • cosmetic ingredients such as dyes, micas and waxes may be used as coating ingredients to improve the appearance and feel of the unit dose.
  • the encapsulation provided for the liquid or granular softening or conditioning materials is preferably a gelatin shell which is readily soluble in the wash water and compatible with detergents used in the wash cycle.
  • the manufacture of such gelatin capsules utilizes technology well known in the art and is described, for example, in the following publications: " Softgels: Manufacturing Considerations", Paul Wilkinson and Foo Song Hom, Drugs Pharmaceutical Science (1990), pps. 409-449, Mediventure Inc., Ann Arbor, MI, USA ; and " Coating of Gelatin Capsules", Ann Mari Hannula and Peter Jardinr, Acta Pharmaceutical Technology (1988), pps. 234-236 .
  • Preferred liquid softeners of the invention include fatty alcohols, such as oleyl alcohol, fatty acids, such as oleyl carboxylic acid; fatty esters, such as oleyl esters or vegetable fatty esters such as sunflower oil ; silicones, such as polydimethylsiloxanes, linear or crosslinked, ethoxylated or without ethoxylation and optionally including an amide functionality; polyethylene waxes, having a molecular weight of from 8,000 to 60,000; and fatty amides, such as dioleyl amide formed by the reaction of diethylene triamine with oleic acid having predominantly the following structure: wherein R 1 represents an oleyl alkyl carbon chain; and R 2 represents H or (EO) x with x varying from 0 to 6 (the degree of ethoxylation).
  • fatty alcohols such as oleyl alcohol, fatty acids, such as oleyl carboxylic acid
  • fatty esters such as oleyl esters or vegetable
  • oleyl carbon chain length is most preferred for purposes of providing softening efficacy and dispersion in the wash water, other higher alkyl chain lengths may also be used for the invention.
  • Typical unit dose compositions for use herein may vary from about 5 to about 10 ml corresponding on a weight basis to about 5 to about 10 grams (which includes the weight of the capsule), and the number of doses per wash is two.
  • the corresponding volume and weight is from about 10 to about 20 ml and from about 10 to about 20 grams (including the capsule weight), respectively.
  • a compacted granular unit dose composition was prepared from the following ingredients: Weight Percent Clay/Pentaerythritol ditallowate (PDT) in a ratio of 83% : 17% 79.97% Effervescent matrix of baking soda and citric acid 17% Polyvinylpyrrolidone 1% Perfume 2% Dye 0.03%
  • This method of manufacture consisted of mixing all the ingredients with the exception of perfume in a Loedige-type mixer. The resulting blend was dried in an oven and perfume was then added to the dried powder. The powder was then compacted using an alternative or rotative press mounted with appropriate dyes. The weight of the spherical unit dose was 60g and such unit dose dispersed in water within 20 minutes when introduced in the wash load at the beginning of the wash in a European Miele W832 front loading washing machine set a Program White Colors at 40°C.
  • the softness provided by the unit dose compositions on terry towels, cotton tee-shirts and cotton kitchen towels was evaluated after cumulative washes and compared with a commercial liquid fabric softener. A 3Kg laundry ballast was used in the machine. Softness was evaluated by a panel of six judges using 9 replicates. The results were as follows: SOFTNESS EVALUATION Laundry Item Softness Comparison Terry towels 1 unit dose softener composition of the invention provided equivalent softness to commercial liquid FS after 10 cumulative wash cycles Cotton tee-shirts 1 unit dose softener provided equivalent softness to commercial liquid FS after one wash cycle Cotton kitchen towels 1 unit dose softener provided enhanced softening relative to commercial liquid FS after one wash cycle .
  • a gelatin encapsulated unit dose liquid softener composition was prepared comprising the following ingredients: Ingredient % (nominal) PDMS (1) 19.00 Trioleate Glycerol 15.00 Sunflower Oil 60.70 Perfume 5.30 (1) Polydimethylsiloxane
  • the softness provided by the unit dose composition was evaluated on cotton tee-shirts and towels in a European washing machine and compared with a commercial liquid fabric softener.
  • the unit dose composition provided essentially equivalent softness.

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Detergent Compositions (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Claims (14)

  1. Einzeldosis-Waschzyklus-Textilweichmacher-Zusammensetzung zum Weichmachen oder zur Konditionierung von Textilien im Waschzyklus einer automatischen Waschmaschine, die aus (a) einer kompaktierten, granulösen Textilweichmacherzusammensetzung oder (b) einer verkapselten flüssigen und/oder granulösen Textilweichmacherzusammensetzung besteht, wobei die Menge von (a) oder (b) zur Bildung einer Einzeldosis ausreichend ist, die ein effektives Weichmachen oder eine effektive Konditionierung der Textilien im Waschzyklus der Waschmaschine erzielen kann, wobei die Textilweichmacherzusammensetzung einen Weichmacherton in Kombination mit einem organischen Fett-Weichmachermaterial umfasst, wobei der Weichmacherton ein Montmorillonitenthaltender Ton und das organischen Fett-Weichmachermaterial eine Pentaerythrit-Verbindung ("PEC") ist, die aus der Gruppe bestehend aus einem höheren aliphatischen Pentaerythritester, einem Pentaerythritoligomer, einem niederen Alkylenoxid-Derivat eines Pentaerythritoligomers und Mischungen davon ausgewählt ist, oder wobei das organische Fett-Weichmachermaterial ein Fettalkohol ist.
  2. Einzeldosis-Weichmacher-Zusammensetzung nach Anspruch 1, dadurch gekennzeichnet, dass sie in Form einer Tablette vorliegt und keine diskrete äußere Schicht aufweist, die den Textilweichmacher umgibt, und aus einem basischen Material besteht, so dass der pH-Wert des Waschwassers bei Auflösung der äußeren Schicht im Waschwasser steigt.
  3. Einzeldosis-Weichmacher-Zusammensetzung nach Anspruch 1, wobei der Weichmacherton mindestens teilweise mit dem organischen Fett-Weichmachermaterial beschichtet ist und als Träger für ein derartiges organische Fett-Weichmachermaterial dient.
  4. Einzeldosis-Weichmacher-Zusammensetzung nach Anspruch 1, wobei der Weichmacherton Bentonit ist und das PEC ein höherer aliphatischer Pentaerythritester oder ein Penterythritoligomer ist.
  5. Einzeldosis-Weichmacher-Zusammensetzung nach Anspruch 1, wobei die Kombination von Ton und Fett-Weichmachermaterial 50 bis 95 Gew.% Bentonit und 5 bis 50 Gew.% PEC umfasst.
  6. Einzeldosis-Weichmacher-Zusammensetzung nach Anspruch 5, wobei die Kombination von Ton und Fett-Weichmachermaterial 80 bis 90 % Bentonit und 10 bis 20 Gew.% PEC umfasst.
  7. Einzeldosis-Weichmacher-Zusammensetzung nach Anspruch 1, wobei der Textilweichmacher einen flüssigen Fettsäureester umfasst.
  8. Einzeldosis-Weichmacher-Zusammensetzung nach Anspruch 7, wobei der Fettsäureester Sonnenblumenöl ist.
  9. Einzeldosis-Weichmacher-Zusammensetzung nach Anspruch 1, wobei die Textilweichmacher-Zusammensetzung ein flüssiges Silikon umfasst.
  10. Einzeldosis-Weichmacher-Zusammensetzung nach Anspruch 1, wobei die Textilweichmacher-Zusammensetzung einen flüssigen Oleylalkohol umfasst.
  11. Verfahren zum Weichmachen oder zur Konditionierung von Wäsche, bei dem die Wäsche mit einer effektiven Menge einer Einzeldosis-Weichmacher-Zusammensetzung kontaktiert wird.
  12. Verfahren nach Anspruch 11, bei dem der Weichmacherton Bentonit ist und das organische Weichmachermaterial eine Pentaerythrit -Verbindung ("PEC") umfasst, die aus der Gruppe bestehend aus einem höheren aliphatischen Pentaerythritester, einem Pentaerythritoligomer, einem niederen Alkylenoxid-Derivat eines Pentaerythritoligomers und einer Mischung davon ausgewählt ist.
  13. Verfahren nach Anspruch 11, bei dem die Textilweichmacher-Zusammensetzung einen flüssigen Fettsäureester umfasst.
  14. Verfahren nach Anspruch 13, bei dem der Fettsäureester Sonnenblumenöl ist.
EP00203113A 2000-04-26 2000-09-08 Wäscheweichspülmittel enthaltende Dosierungseinheit zur Verwendung in einem Waschgang Expired - Lifetime EP1149893B1 (de)

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Application Number Priority Date Filing Date Title
EP05076606A EP1586626A3 (de) 2000-04-26 2000-09-08 Wäscheweichspülmittel enthaltende Dosierungseinheit zur Verwendung in einem Waschgang

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US09/558,822 US6258767B1 (en) 2000-04-26 2000-04-26 Spherical compacted unit dose softener
US558822 2000-04-26
US620515 2000-07-20
US09/620,515 US6294516B1 (en) 2000-04-26 2000-07-20 Wash cycle unit dose softener

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EP05076606A Division EP1586626A3 (de) 2000-04-26 2000-09-08 Wäscheweichspülmittel enthaltende Dosierungseinheit zur Verwendung in einem Waschgang
EP05076606.2 Division-Into 2005-07-12

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EP1149893A1 EP1149893A1 (de) 2001-10-31
EP1149893B1 true EP1149893B1 (de) 2010-12-15

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US6589930B2 (en) 2003-07-08
US20020013244A1 (en) 2002-01-31
US6291421B1 (en) 2001-09-18

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